Process of and apparatus for neutralizing oils



Mar. 6, 1923. 1,447,898.

' H. SCHLOSSSTEIN.

PROCESS OF AND APPARATUS FOR NEUTRALIZING OILS.

FILED JUNE 26. 1919.

HANS SCHLOSSSTEIN,

T T OFFICE.

or CHICAGO, ILLINOIS.

PROCESS OF AND APPARATUS FOR NEUTRALIZING OILS.

Application filed .Tune 26, 1919. Serial No, 306,799.

T 0 all whom it may concern:

Be it known that I, HANS SoHLosssTEIN, a subject of the Government of Germany,

and a resident of Chicago, in the county of Cook and State of Illinois, have invented certain new and useful Improvements in Processes of and Apparatus for Neutralizing Oils; and I do hereby declare thatthe followin is a full, clear, and exact descriptionthereof, reference being had'to the accompanying drawings, and to the characters of reference marked thereon, which form a part of this specification.

This invention relates to a novel process' of and apparatus for neutralizing fixed fatty acid oils or the synthetic formation of neutral fats.

Among the objects of the invention is to provide a novel process of and apparatus for the purpose set forth which is attended with little or no refining losses; to provide a process that will accelerate the operation and thereby reduce its cost; to provide a process of and apparatus for neutralizing oils having a high free fatty acid content which cannot be practically neutralized by known neutralizing processes on account of the resulting high refining losses; to provide a process by which it becomes possible to convert pure fatty acids into neutral oils,

yto make possible the utilization of fats which heretofore have found a very limited use, and also to extract glycerinfro'm the cheaper fats and reconstruct thereby the more expensive fats.

In practicing my novel process a quantity of oil or fatty acids to be treated is charged into a vacuum kettle in whichthe material is maintained at the desired temperature.

The material is delivered, as by means of a suitable pump, to a mechanical emulsifier,

where it is mixed with an emulsifying agent to rapidly emulsify the mixture, a treating agent, and with a solvent for all the constituents, wherea-t the liquids meet under pressure and the formation of fat takes place. The emulsifying agent may be a small percentage of aromatic sulpho-fatty acid, such as is known, for instance, as 'iwitchell reagent. The treating agent is a multi-atomic alcohol, such as glycerin or 'lyCOl of a percentage due to the character of the treated material, and the solvent may be either acetone or alcohol. The emulsifying agent is not soluble in the treated material and the treating agent, but the solvent material to be treated, and the treating agent.

A required amount of glycerin, practically equivalent to the theoretical or known quantity necessary .such as is hereinafter suggested, is mixed with the other ingredients, acetone or alcohol and aromatic sulphofatty acids, ina container which is in communication with the emulsifier, and said container is preferably under a carbon dioxide or hydrogen pressure, and may be cooled if desire i The mixed liquids are projected from the emulsifier, which is rotated at high speed, 'undei' centrifugal force, and is released from a state of pressure in a fine spray in .a

vacuum, the combined act-ion of the cen-" trifugal force, the sudden reduction of pressure and the relative higher temperature of the vacuum space serving to very finely subdivide the mixture. The acetone or alcohol, together with water which has been formed, will be quickly drawn from the vacuum space by reason of the sudden release of pressure and the ruling temperature and the elements desired to be recovered may be externally recovered in a condensate container. The emulsion resulting from the mixture of the fatty acids, the emulsifying agent, and the treatin agent are thereafter mixed, at a second stage, with a second supply of fatty acids, bein brought to ther in a mixing device which dissolves the emulsion in the fatty acids or oil. Said mixing device may comprise a. rotative casing having a screen-like cylindric wall through which the emulsion and the fatty acids are thrown by centrifugal action in the form of a fine spray. the treatment continuing until complete transformation of the fatty acid into fat has been obtained. At the prevailing temperature and pressure the glycerin or treating agent is in a condition particularly active for intimate contact with the fatty acid, thus reducing thetime of operation. Any moisture that may be formed will be drawn off immediately through a vacuum connection with the space into which the mixture is sprayed, and any portion of the glycerin or glycol that should go over with the moisture may be recovered in an external condensate container. Inasmuch as the mixture of the emulsion with the fatty acids or oils at the second stage takes place in a vacuum, the moisture will thus be instantly removed from the material, thereby preventing reversal of the process which otherwise might occur if the mixture were allowed to remain. After the formation of fat is completed the sulpho-fatty acids may be removed by saponification or washing by acetone.

By reason of the active mechanical emulsification under pressure and by reason also of the fact that the emulsifying agent and treating agent are furnished in a solution which serves as a common solvent forthe emulsifying agent, the material to be treated and the treating agent, a very small percentag of the emulsifying agent, such as aromatic sulpho-fatty acids, need be used, and, therefore, need beremoved from the finished product. The mixture of the fatty acids from the vacuum kettle with the emulsion from the emulsifier takes place preferably at a temperature higher than the emulsifying temperature and at a temperature and correlative pressure which renders the action of the treating agent, as glycerin or glycol, particularly effective. The second stage mixing device may be practically operated by the same motor or driving device that drive the movable element of the mechanical emulsifier.

Preferably and as herein shown, the treatment of the oil or fatty acid may take place in a single receptacle under a high vacuum, the fatty acids" from the receptacle being raised to the emulsifier and the mixing device and allowed to pass back into the lower part of the receptacle for treatment until the material has been fully treated.

I have shown in the drawings one practical apparatus for practicing my process, and will describe the same in connection with a more specific recitation of the steps of the process.

The figure of the drawing is a verticalsection of an apparatus .for practicing my process.

As shown in the drawings, 10 designates a vacuum kettle, the contents of which may be heated by a steam jacket 11 or by any other suitable source of heat. The kettle terminates at its upper end in an enlarged flaring chamber 12 which is closed by a top wall 14:

and may be heated by a continuation of the steam jacket or other suitable heating means.

28 designates a funnel-like partition that separates the upper from the lower part of the chamber 12 to produce an upper compartment 34: and a lower compartment 35. Said diaphragm'28 extends from the upper larger end of the chamber 12 toward the center of the chamber and is formed at its center with an opening 29.

At the top of the chamber 12 is located a mechanical emulsifier. It comprises an upper fixed element 16 and a lower rotating element 17, the proximate faces of the eleraa'aeee ments being of suitable or known formation and closely spaced to closely divide the materials therebetweem' between which the liquid is emulsified. Said rotating element is shown as operated by a motor 18, or other driving mechanism, fixed in the top of the kettle l0 and is connected to the rotating element by a shaft 19. The motor may be an electric motor or a steam turbine and is enclosed by a suitable shell or housing. The fixed element 16 of the mechanical emulsifier has a central feed opening to which is connected a pipe 20 that leads from a tank 21 suitably supported above the wall 14. Through said feed opening the mixture of the emulsifying agent, the treating agent, and the solvent is fed to the emulsifying space between said members.

A portion of the fatty acid to be treated may be forced from the bottom of the kettle 10, as by means of a pump 22 operated from an exterior source of power by a shaft 23, through a pipe 24, the outlet end 25 of which discharges into the receiving inlet of the mechanical emulsifier. Preferably, and as herein shown, said pipe 2st includes a cooling coil 26 that is contained in a cooling chamber 27 through which a cooling agent, as water, may be passed to cool the contents of the pipe 24: before being discharged into the mechanical emulsifier.

Below the opening 29 of the partition 28 and as herein shown, supported on and ro tated by the shaft 19, is a second stage mixing device 30 which comprises a cylindric shell having imperfor ate top and bottom walls, except for a central opening in the top wall, and a screen-like cylindric side wall 31. 32 designates a pipe which extends from a second delivery opening of the pump 22 and upwardly through the diaphragm 28 and is provided above said diaphragm with a down-turned nozzle 33 which discharges into the central opening 29 of the diaphragm 28.

The upper and lower compartments 34, 35 of the chamber, as well also as the kettle. are connected to a common vacuum pipe 36 which leads to a vacuum pump, not shown, whereby a high vacuum may be maintained in both said compartments. I

The operation of said apparatus to practice my novel process is as follows:

A quantity of fixed fatty acids, such as cocoanut oil fatty acids to be treated is charged into the kettle 10 to at approximately the level indicated by the dotted line a and isheated by 'the steam jacket. The pump 22 and the driving device118 are set in operation, the latter operating through the shaft 19 to rotate the mechanical emulsifier 15 and the mixing device 30. The speed of rotation of said emulsifier and mixing deminute. The pump 22 which may be a centrifugal pump, operates through one discharge to force the oil or fatty acids from the bottom of the kettle through the pipe 24 to the mechanical "emulsifier and also through another discharge and the pipe 32 to the central opening 29 of the upper coin-' partment 34. The oil or fatty acids may be maintained at a temperature in the kettle of from 175 to 225 C. the oil as it passes through the pipe 24 to the emulsifier is reduced by its passage through the cooling coil 26 and is delivered at the mechanical emulsifier at a temperature of about 100 to 150 degrees C. and at a pressure due to that maintained in the tank. A high vacuum is maintained in the compartments 34, 35 and in the kettle. The

tank 21 has theretofore been charged with a tral inlet opening of the fixed element 16 of the mechanical emulsifier into the emulsifying space thereof along with the solvent, the emulsifying agent and treating agent from the tank 21. The liquids meet in the emulsifier under pressure and at a tempera ture below that in the kettle andv the for-mation-of fat takes place. By reason of the cooling means employed the temperature of the mixture at the emulsifier 15 is kept below the evaporating point of the solvent under the prevailing pressure.

The high-speed of rotation of the rotative element and thepeculiar formation of the emulsifier elements intimately intermixes the fatty acids with the solvent, the emulsifying agent, and treating agent so as to materially reduce the quantity of the emulsifying agent required. The emulsion is thrown outwardly by centrifugal force and, by reason of the sudden reduction of the pressure and of the small outflow openings, in the form of a fine spray against the funnel-shaped diaphragm '28 and flows downwardly over the inclined diaphragm to the central opening 29. Moisture in the sprayed emulsion and also the solvent agent is withdrawn by reason of the vacuum.

The emulsion is further mixed at the second mixing stage in the mixing device 30 with the oil or fatty acids'that are conducted to the feed opening 29 through the pipe 32 and the resultant mixture is thoroughly agitated and mixed by the high rotation of the mixing device 30. The emulsion will readily dissolve in the oil delivered The temperature of through the pipe 32, the mixture being thrown by centrifugal force through the screen wall of the mixing device 30in the form of a fine spray and falls into the kettle 10. Any moisture formed at this stage will be drawn oif immediately through the vacuum and eventually also parts of glycerin that may go over with the mixture will. be recovered in an external concentrate con tainer.

By reason of the intimate commingling of the oil or fatty acids and the emulsion in the mixing device 30, and of the fact that the.

mixture is thrown outwardly by centrifugal action through thefine mesh of the screenvlike wall 31, and becausealso at the prevailing temperature in the compartment 35 the glycerin is in a particularly active stage and is in'such physlcal condition as to be in most intimate contact with the fatty acid mole cules, an intimate intermixture of the materials is insured, thus increasing the efficiency and reducing'the time of operation. The mixture of the oil or fatty acids delivered through the pipe 24 with the solvent, treating, and emulsifying agents from pressure tank 21 takes place under apressure that will hold the solvent from evaporating while in the emulsifier, and this pressure is immediately released the moment the mixture leaves the emulsifier and is sprayed in the vacuum compartment 34, and insures the immediate removal of the water that may be produced in the process of the fat formation. So also water formed in the second stage of the operation is withdrawn by the existing vacuum. If this water be not removed at the moment of its formation a reversal of the process. forming fatty acids, would be liable to occur. Furthermore, the carrying out of the process in the vacuum safeguards the treatment of the oil with respect to its taste inasmuch. as it would be impaired in this regard by the temperature if the process were carried outin. the presence of air or in the presence or other gases. The presence of air or other gases would also render difficult the immediate removal of the moisture at the time. of its formation and would, therefore, considerably delay the carrying out of the process and would also impair the activity or the glycerin or treating agent.

Anexample of the material treated and the proportions of the treating. emulsifying, and solvent agents which have been. in practice, proven efficient may be stated as follows:

Assuming 100 pounds of cocoanut oil fatty I the container 21. As before stated, a pressure is maintained in the container 21, so as to deliver the mixture of treating, emulsifying, and solvent agents to the space between the elements of the mechanical emulsifier at a. substantial pressure correlative to the temperature of the aforesaid mixture and the temperature of the incoming material being treated, that is delivered through the pipe 24. The elements of the emulsifier are so closely spaced and are roughened on their proximate sides, as shown in thedrawings,

' tures specified, By reason of this pressure and the relatively low temperature between the emulsifier elements, and of the high temperature and vacuum into which the mixtu e is sprayed from the emulsifier elements, the water and solvent agent will be instantly taken up by the vacuum and removed.

In practice, it has been found that with a batch of material, such as herein suggested, after being treated for a period of about two hours, substantially 85 per cent of the fatty acids have been transformed into neutral fats and after about four hours treatment, substantially all of the fatty acids have been transformed into neutral fats.

Another advantage of the process is that the glycerin, oils, or fatty acids and aromatic sulpho-fatty acids do not dissolve each in the other, but the acetone or alcohol. constitutes a common solvent for all three constituents. thus insuring a very intimate contact of thethre-e liquids, which, in turn, accelerates the process. For this reason it is possible to use a very much smaller quantity of aromatic sulpho-fatty acid than in known oil neutralizing processes; The acetone or alcohol and eventually also small parts of the glycerin which have been evap orated will be condensed and recovered in a condensate container so that, therefore, there is no actual loss in the entire operation,

I claim as my invention:

1. The improvement in the pro ess of neutralizing fixed fatty acid oils, which comprises the step of mixing the material with an emulsifying agent and a multi-atomic alcohol in the presence of a solvent common to all.

2. The improvement in the process of neutralizing fixed fatty acid oils. which comprises the steps of mixing the material to be treated with an emulsifying agent and a multi-atomic alcohol in the presence of a intimately mixing 1 ,amgsas prises the steps of mixing the material to be treated with an emulsifying agent, 'a multiatomic alcohol, and a solvent there-for while under pressure. and rapidly emulsifying the mixture and spraying the: emulsion in a vacuum.

5. The improvement in the process of neutralizing fixed fatty acid oils, which comprises the steps of mixing the material to be treated at one stage with an emulsifying agent and multi-atomic alcohol in the pres- 'ence of a common solvent, and thereafter mixing the. resultant emulsion at another stage with said material in a vacuum.

6. The improvement in the process of neutralizing fixed fatty acid oils, which comprises the steps of'mixing the material to be treated at one stage with an emulsifying agent and a multi-atomic alcohol, rapidly emulsifying the said mixture under pressure, releasing said pressure, and thereafter mixing the resultant emulsion at another stage with another supply of said material in a vacuum.

7. The improvement in the process of neutralizing fixed fatty acid oils, which comprises the steps of mixing the material to be treated at one stage with an emulsifying agent and a multi-atomic alcohol. rapidly emulsifying the said mixture under pressure, releasing said pressure, and thereafter mixing the resultant emulsion at another stage with another supply of said material at a temperature to stimulate the action-of the alcohol.

8. The improvement in the process of neutralizing fixed fatty acid oils, which comprises the steps of mixing under pressure the material to be treated with an emulsifying agent and a multi-atomic alcohol in the presence of a common solvent and thereafter rapidly emulsifying said mixture and discharging it in a vacuum.

9. The improvement in the process of.

H ll

neutralizing fixed fatty acid oils, which com prises the steps of mixing the material with an emulsifying agent and a multi-atomic alcohol under pressure": in the presence 0 a common solvent, emulsifying said mixture, the resultant emulsion with another supply of the material in a vacuum, and reducin the temperatureof the-material delivered to the emulsifier to reduce the emulsifying temperature.

10. The process of neutralizing fixed fatty acid oils, which comprises the steps of heating a body of material in vacuum, mixing a portion of the said material with an emulsifying agent, a multi-atomic alcohol, and with a solvent common to all, subjecting the mixture to an emulsifying process under pressure, and releasing the emulsion in a vacuum and allowing it to flow back into the body of said material.

11. The improvement in the process of neutralizing fixed fatty acid oils, which comprises the steps of mixing under pressure the material to be treated with an emulsifypresence of a common solvent, and thereafter rapidly emulsifying said mixture.

12. Apparatus for-neutralizing fixed fatty acid oils comprising a receptacle to receive the material to be treated, means to heat the material in said receptacle, means to maintain a vacuum therein, a rotative mechanical emulsifier and spraying device in said receptacle, and pressure means to deliver to said emulsifier said material from the receptacle, together with an emulsifying and a treating agent and a solvent common to both said emulsifier having means to co-operate with said pressure means to maintain substantial pressure on the material and to suddenly release said pressure. J

13. Apparatus for neutralizing fixed fatty acid oils comprising a receptacle to receive the material to be treated, means to heat the material in said receptacle, means to maintain a vacuum therein,-a rotative mechanical emulsifier and spraying device in said receptacle. means to deliver under pressure said material from the receptacle together with an emulsifying and a treating agent and a solvent common to both, and a second stage mixing device in said receplng agent and a multi-atomic alcohol in the tacle to which the emulsion from the emulsifier is delivered, with means for delivering material to said mixing device and intimately intermixing it with the emulsion.

14. .Apparatus for the purpose of neutralizing fixed fatty acid oils comprising a receptacle to receive the material to be treated, means to heat the material in said receptacle, means to maintain a vacuum the-rein,

said receptacle being provided at its top with an internal conical diaphragm, a rotative mechanical emulsifier in said receptacle, having means to receive material to be treated, together with a treating agent, an emulsifying agent and a solvent common to all, said emulsifier operating to spray the emulsion outwardly against the upper side of said being collected at an opening in the center of the dia hragm, and a second stage mixing device eneath said diaphragm to receive and,intimately intermix the emulsion with said material.

In testimony whereof I claim the foregoing as my invention, I hereunto append my signature at Chicago, Illinois, this 20th day of June, 1919. p HANS SCI-ILOSSSTEIN. 

